Two-dimensional 1H NMR of three spin-labeled derivatives of bovine pancreatic trypsin inhibitor.
Two-dimensional 1H NMR of three spin-labeled derivatives of bovine pancreatic trypsin inhibitor.
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牛胰蛋白酶抑制剂的三种自旋标记衍生物的二维 1H NMR。
DOI：
10.1021/bi00357a009
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发表时间：
1986
期刊：
影响因子：
2.9
通讯作者：
Kuntz,ID
中科院分区：
文献类型：
--
作者：
Kosen,PA;Scheek,RM;Naderi,H;Basus,VJ;Manogaran,S;Schmidt,PG;Oppenheimer,NJ;Kuntz,ID
药物化学系，加州大学，弗朗西斯科，加州94143接收于1985年10月21日;修订的Mandarin pt接收于1985年12月19日摘要：用氨基特异性试剂琥珀酰亚胺1-氧基-2，2，5，5-四甲基-3-吡咯啉-3-羧酸酯制备了三种氮氧自旋标记的牛胰蛋白酶抑制剂单衍生物。通过离子交换和亲和色谱法纯化单衍生物。的单衍生物的胰蛋白酶肽的薄层地图显示，自旋标记被纳入在任一a-氨基，赖氨酸-15，或赖氨酸-26。记录单衍生物的二维1H NMR谱。用抗坏血酸还原氮氧自由基标记物生成羟胺后也记录了光谱。与氮氧标签的存在下，显着的谱线加宽的影响，在光谱中的许多交叉峰进行了观察。CnH-NH交叉峰的谱线增宽程度与晶体结构中标记的氨基和平均CnH-NH位置之间的距离定性相关。自旋标记影响~ 15 A内质子的交叉峰。这项研究表明，它是可行的，积累足够的分子内距离，以确定蛋白质溶液的结构与距离几何算法的帮助。高场二维核磁共振谱的出现，使人们对以与X射线晶体学相当的分辨率获得大分子的时间平均溶液构象产生了新的兴趣。Wiithrich和他的同事们开创了核Overhauser效应、邻位耦合常数和从二维光谱获得的氢交换速率的组合使用，以鉴定蛋白质中二级结构的区域（瓦格纳& Wiithrich，1982 b; Hosur等人，1983; Pardi等人，1983;威廉姆森等人，1984年）。作为一种补充方法，他们建议使用从NOESY实验中获得的氢-氢空间距离与距离几何计算（Havel等人，1979，1983; Havel & Wiithrich，1985）以确定蛋白质的三维结构（Braun et al.，1981，1983; Wiithrich等人，1982;威廉姆森等人，1985年）。其他人也做了类似的
Department of Pharmaceutical Chemistry, University of California, San Francisco, California 94143 Received October 21, 1985; Revised Manuscript Received December 19, 1985 abstract: Three nitroxide spin-labeled monoderivatives of bovine pancreatic trypsin inhibitor were prepared with the amino-specific reagent succinimidyl l-oxy-2, 2, 5, 5-tetramethyl-3-pyrroline-3-carboxylate. The monoderivatives were purified by ion-exchange and affinity chromatography. Thin-layer maps of tryptic peptides of the monoderivatives showed that the spin-label was incorporated at either the a-amino group, Lys-15, or Lys-26. Two-dimensional/-correlated’H NMR spectra of the monoderivatives were recorded. Spectra were also recorded after reduction by ascorbic acid of the nitroxide labelto hydroxylamine. With the nitroxide label present, significant line-broadening effects on many of the cross peaks in the spectra were observed. The extent of line broadening for the C «H-NH cross peaks was qualitatively correlated with the distance between the labeled amino group and the average C „H-NH position in the crystal structure. The spin-label affects cross peaks of protons within~ 15 A. This study suggests that it is feasible to accumulate sufficient intramolecular distances in order to determine protein solution structures with the aid of distance geometry algorithms. e advent of high-field two-dimensional NMR1 spectroscopy has created a renewed interest in obtaining time-averaged solution conformations of macromolecules at a resolution comparable to that of X-ray crystallography. Wiithrich and his colleagues pioneered the combined use of the nuclear Overhauser effect, vicinal coupling constants, and hydrogen exchange rates obtained from two-dimensional spectra to identify regions of secondary structure in proteins (Wagner & Wiithrich, 1982b; Hosur et al., 1983; Pardi et al., 1983; Williamson et al., 1984). As a complementary approach, they have suggested using hydrogen-hydrogen through-space dis-tances obtained from NOESY experiments in conjunction with distance geometry calculations (Havel et al., 1979, 1983; Havel & Wiithrich, 1985) to determine the three-dimensional structure of a protein (Braun et al., 1981, 1983; Wiithrich et al., 1982; Williamson et al., 1985). Others have made a similar
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单克隆抗自旋标记抗体的磁共振
影响因子：
2.9
作者：
J. Anglister;T. Frey;H. Mcconnell
通讯作者：
H. Mcconnell
神经毒素衍生物与乙酰胆碱受体或单克隆抗体的相互作用。
DOI：
10.1111/j.1432-1033.1984.tb08063.x
发表时间：
1984
期刊：
European journal of biochemistry
影响因子：
--
作者：
A. Rousselet;G. Faure;J. Boulain;A. Ménez
通讯作者：
A. Ménez
影响因子：
--
作者：
C. Hirs
通讯作者：
C. Hirs
距离限制对大分子构象的影响。
DOI：
--
发表时间：
1979
期刊：
影响因子：
--
作者：
Timothy F. Havel;G. Crippen;I. Kuntz
通讯作者：
I. Kuntz
通过二维 1H NMR 动态过滤并应用于噬菌体 lambda 阻遏物。
DOI：
10.1073/pnas.81.19.6019
发表时间：
1984
影响因子：
11.1
作者：
Weiss,MA;Eliason,JL;States,DJ
通讯作者：
States,DJ